FR2702779A1 - Obtaining denim textiles with an overdyed and washed out appearance. - Google Patents

Abstract

The invention describes a one-bath process for imparting both a washed out and overdyed appearance to denim textiles and to denim articles. The single bath comprises a dye, a cellulase enzyme, optionally, but preferably, a salt and / or an amylase.

Description

The present invention relates to the treatment of dyed textiles and,

  more particularly, obtaining textiles in

  jeans with an overdyed and washed out appearance.

  The dyed cellulosic textiles that we know cover

  under the name of "jeans" are used to manufacture a wide variety of products, in particular clothing such as "blue jeans", skirts, jackets, shirts,

  as well as other products such as bags and holders

  currency Denim textiles (or simply ujean ") are generally constructed of a warp thread which is woven with a weft thread Generally, the warp thread is dyed in a color such as indigo, blue, black or another color, while the weft thread is generally an unbleached or white thread We also know denim textiles in which

  both warp and weft thread are dyed.

  There are three methods that are commonly used to obtain fashionable and / or aesthetic finishes on jeans. These are "1 wash", nsurteinturen and a combination of these two to give what 'we call it, miserable look ". We wash out by washing the jeans in the presence of an abrasive substance (typically pumice), by treating the jeans in a bath comprising at least one cellulase enzyme, under suitable conditions , or by a combination of these two treatments Desizing can

  take place or accompany the abrasion process La surtein-

  ture consists in subjecting the jeans which have already been dyed, in particular jeans comprising an undyed weft thread, to a dyeing process, usually with a direct dye,

  under appropriate dyeing conditions.

  The "miserable look" is obtained by a washing (enzymatic and / or abrasive), followed by an overdyeing The resulting products are more flexible and attractive and one can obtain attractive coloring effects However, the production i of a result so attractive has so far required the use of a series of two stages, each with specific requirements, which makes the industrial process

  relatively complicated and expensive.

  We have now discovered, surprisingly, that it is possible to obtain an attractive appearance on jeans by a process involving a single bath and which is ultimately easier to implement and less expensive. The invention The invention therefore further provides an aqueous treatment bath for textiles, comprising at least one dye which is effective for providing a process for the treatment of a denim textile, comprising treating the textile with a cellulase enzyme in the presence of a dye. dyeing textiles or textile articles containing cellulose, preferably jeans, and at least one enzyme active against cellulose, effective in imparting a wretched or washed-out effect to textiles or textile articles containing cellulose, preferably jeans The process according to the invention can be incorporated into processes for treating conventional denim textiles, in particular processes which aim to work iter jean textiles or jean items

  to give them an over-colored and miserable (or washed-out) appearance.

  The present invention also provides a preparation for

  the treatment of textiles comprising at least one dye ef-

  effective for dyeing textiles or textile articles containing cellulose, preferably jeans, and at least one enzyme active against cellulose, effective in imparting a miserable or washed-out effect to textiles or fabrics

  textile articles containing cellulose, and possibly-

  Lement, but preferably a salt.

  The present invention further provides a method of treating denim textiles which consists of carrying out a simultaneous treatment with amylase (desizing of starch) and with cellulase in the presence of a dye which removes the

  need for a separate desizing step.

  The present invention further provides a preparation for the treatment of textiles comprising at least one dye effective for dyeing textiles or textile articles comprising cellulose, preferably jeans, and at least one enzyme active against cellulose, effective in imparting a wretched or washed-out effect to textiles or textile articles containing cellulose, an amylase

  desizing of the starch and, possibly, but of pre-

ference, a salt.

  Other characteristics of the invention will appear

  better on reading the detailed description that follows.

  Cellulose-active enzymes also known in the art as Cellulases ", which are useful in the practice of the present invention, include compositions and preparations containing an enzyme active against cellulose screws which are well known

in the textile industry.

  A wide variety of these compositions is available and suitable for practicing the present invention.

  compositions and preparations containing an active enzyme vis-

  cellulose may contain a mixture of cellulases produced from a natural source, such as a microorganism, or may contain one or more cellulose-decomposing enzymes, which have been produced by a

  recombinant technology Typically, the compositions containing

  a cellulose active enzyme employs endocellulases or mixtures thereof which include at least about 50% endo-cellulases and other cellulases

  breaking down cellulose, including exo-cellulases.

  Other cellulase enzymes which act on the enzymatic breakdown products of cellulose may also be

  present, e.g. cellobiohydrolase and / or cello-

  biase. It is well known that cellulose enzymes present their

  action optimally or only under certain conditions

  p H and temperature and are also subject to deactivation in the presence of various elements or substances In general, cellulase enzymes exhibit activity in the p H range of 3.8-6.5 and in the range for temperatures of 35-65 C. For reasons of definition in the present invention, the optimal activity is defined as being a condition of p H and / or of temperature which makes it possible to obtain at least 50% of the maximum activity A domain of p H of optimal activity is a domain of p H in which the enzyme exhibits this optimal activity independently of the temperature A range of temperatures of optimal activity is a range of temperatures in which the enzyme exhibits this optimal activity independently of the p H When carrying out the process of the invention, the cellulose is chosen so that its general activity in terms of p H and of temperature is judged satisfactory with regard to the res ultats with the particular dye chosen for use For the purposes of this invention, cellulases exhibit their optimal activity in the field

  of p H of 3.8-5.5 and in the temperature range of 55 -65 'C.

  The quantity of cellulose enzyme used depends largely on the length of the treatment desired, the treatment conditions and the final effect sought. Expressed in units of cellulase activity, the quantity of cellulase enzyme used can vary over a wide range, by example of 900 CMC units per pound (0.454 kg) of fabric, up to approximately 6000 CMC units per pound (0.454 kg) of fabric, or even more Preferable amounts of 1500 to 6000 CMC units per pound can generally be used (0.454 kg), and amounts of about 2000 to about 3500 units per pound (0.454 kg) can be used during the most conventional treatment periods, for example 35-50 minutes to achieve good results with considerable reduction white stripes

  and good final product quality.

  Generally, for the most popular treatments, the quantity of cellulase enzyme used is in the range that is commonly used to abrade textiles under conditions of p H, time and temperature which are normally associated with the cellulase enzyme in the absence of dye A conventional set of processing conditions encompasses the presence of cellulase enzyme in the range of about 2000-3000 CMC units per pound (0.454 kg) of textile, over a treatment period of 15-60 minutes A suitable processing temperature is a range of temperatures in which the cellulase enzyme is sufficiently active to impart the washed-out effect, which is recognized to be dependent on the particular cellulase enzyme used Conventionally, a temperature between about 55 'C

and about 60 C is effective.

  Amylase enzymes, also known in the art as "amylases", which are useful in the practice of the present invention, include compositions and preparations containing an amylase enzyme which are well known in the textile industry. variety of these compositions are known and are available and considered suitable in the practice of the present invention These compositions and preparations may contain a single amylase or may be in admixture with cellulases produced from a natural source, such as a microorganism, or may contain one or more cellulose-decomposing enzymes that have been produced by a

recombinant technology.

  As is known in the art, delivery agents

  starch-based bonding includes both those which are in the form of starch and those which are in the form of starch with other starch-type sizing substances, such as polyvinyl alcohols, polyvinyl acrylates and / or carboxymethylcellulose Usually, the latter form of sizing agents comprises at least approximately 30% by weight of starch, but more commonly comprises at least approximately 50% by weight of starch The amylases used in the implementation of certain Embodiments of the invention may be used in any quantity, but are advantageously used at least in a minimum amount effective to substantially decompose the starch portion of

  the sizing agent present on the textile to be treated.

  The expression "substantially decompose%" means that at least about 80% by weight of the starch present in the starch-based sizing agent will be eliminated by the amylase, or better still at least 90% will be eliminated. tests to determine the amount of added starch that is removed in a conventional desizing step are well known in

  industry and can easily be used to determine

  undermine the minimum effective amount of amylase enzyme required

  to decompose substantially the sizing agent to

starch base.

  As will be realized by a person skilled in the art, the effectiveness of the amylase is largely a function of the concentration and the time, for a given operating condition, such as p H and temperature. To implement the process of the invention , it is desirable that the amylase and its quantity be chosen so that it exhibits a sufficient advantageous activity under the conditions of the bath in which it is used, so that the sizing agent is substantially decomposed, as described above It is understood, however, that the total contact time of the amylase and the textile material will be longer than expected if the amylase is used essentially only in one step desizing, it should be expected that the total amount of amylase, when used in conjunction with the cellulase and the dye according to the invention, may be less than the amount that would be required in a process step. separate desizing process If a treatment composition based on a representative amylase enzyme having a concentration and an activity of which the types are well known in the industry is used, for example Bactosol MTN (available from Sandoz Chemicals, Basel , Switzerland), an amount of at least 0.4 g per liter will usually be used. Although amounts as high as 4 grams per liter of treatment bath (and even more) can be used, it is generally preferred to use about 0.5 to 2 g per liter of bath, better still 0.75 to 1.5 g per liter. Dyes which are useful include water-soluble or water-dispersible dyes which are useful for dyeing cellulose, for example direct dyes and reactive dyes for fibers. Preferably, the dyes are direct dyes Those which are useful for the invention are direct dyes which are well known in the art and which include those which are defined in the Color Index, volume 2, pages 2005-2478 (The Society of Dyers and Colorists, London, 1971), the contents of which are incorporated herein by reference. Most direct dyes belong to the classes of diazo, triazo and polyazo compounds, while the

  minority of direct dyes are classified in the

  tegories of monoazo dyes, stilbene, oxa-

  zine, thiazine and phthalocyanine Usually, direct dyes have an anionic character compared to cellulose and are applied from the aqueous bath containing an electrolyte Such an electrolyte is generally formed by adding, in the dye bath, '' at least an effective amount of a salt generally used in conjunction with a direct dye More frequently, the salt is sodium chloride, sodium sulfate or sodium sulfate

  sodium decahydrate (Glauber's salt).

  According to the teachings of the invention, there is provided a process for treating denim textiles or articles containing denim textiles which serves to impart to them simultaneously a washed-out appearance and an over-dyed appearance. The process is advantageously used on upholstery textiles. dyed jeans as well as articles containing such denim textiles dyed or made from such textiles Denim textiles may be in an unsewn or partially sewn state, or in a fully finished product state Denim textiles which are composed of less than 100% cellulose fibers, as is the case of mixtures of fibers which contain both cellulosic fibers and non-cellulosic fibers, can also be treated by the process of the invention These fibers can be incorporated in the weft thread or in the dyed warp thread, or in both Examples of these denim textiles containing less than 100% of fibersd cellulose are those which are called Istretch K blends which can be, for example, blends which comprise 65% cotton and 35%

  synthetic polyester fibers The process is advanced

  taggedly implemented with dyed denim clothing which is also found in the form of finished products. In particular, clothing such as pants,

  jeans, skirts, shirts and jackets.

  According to one aspect of the process of the invention, the jean textiles are brought into contact, in a single aqueous bath which comprises effective amounts of a cellulase enzyme, of a direct dye and of a salt, under conditions which allow the action of the cellulase enzyme and

  direct dye used both to decompose and to

dye the denim textile.

  According to another method of the present invention, the jean textiles are preferably first desized The desizing of a jean textile can be done according to conventional techniques, in particular the contacting of the jean textiles with one or more baths containing desizing agents, such as desizing agents

  conventional or an effective amount of an amylase enzyme.

  According to another aspect of the invention, denim textiles do not have to be first desized if using amylases and cellulases according to certain

  methods of the present invention.

  The relative proportions of the constituents used according to the single-bath process described here must be understood as being variable - over a wide range and are in large

  part depending on the final treatment of the textile to be carried out.

  The variables to be considered include the operating conditions such as time, temperature, concentration, as well as other conditions which may depend on the process and / or the apparatus to be used. Other variables affecting the quantity of constituents include considerations relating to the particular constituents chosen, such as the particular preparation of cellulase enzyme and the direct dye chosen Other considerations depending on the desired end product include the final degree or the final depth of the desired dye and the final degree of softening of the textile or of washed-out effect which must be imparted to the textile by the treatment process These relative proportions can be determined by a routine experimental evaluation. By way of nonlimiting example, various illustrative operating conditions, as well as unique bath compositions are given in

  the examples described in detail below.

  The treatment baths may also contain other constituents which are conventionally used in the technique of treating textiles. By way of example, but not by way of limitation, mention may be made of wetting agents, setting agents suspension, dispersants, surfactants, leveling agents, buffering agents, and the like One or more of these additives can be added to the single baths according to the invention in any amount which does not appear to undesirably limit the

  functioning of the cellulase and the direct dye and,

amylase.

  The treatment baths may contain an acid and / or a buffer to establish or regulate the p H of the single bath so that it is within the effective p H operating limits of the particular cellulase enzyme selected A bath may be formed by adding the direct dye and salt to water, after which a sufficient amount of acid is added to the single bath to adjust the p H so that it is within the effective working range of p H of the cellulase enzyme and of the amylase enzyme, optionally present The specific enzymes are then added to the single bath Then a buffer can be added to the bath, in an amount sufficient to regulate p H substantially in the p domain H in which the cellulase enzyme has at least its optimal activity For this purpose, the useful acids include mineral or organic acids Particularly contemplated as useful acids are organic acids such as acetic, citric and oxalic cides As useful buffering agents, conventional buffering agents are contemplated, especially monosodium buffering agents such as buffering agents containing sodium acetate, sodium carbonate, sodium phosphate and sodium hydroxide. sodium The conventional effective quantities range from 1 to 6 g per liter of water in the single bath. These quantities are very particularly in the range of 2 to 4 g per liter of water. Another useful constituent which can be incorporated into the bath is a surfactant. The surfactants advantageously have a good detergent action and can be of the nonionic, amphoteric and / or anionic type. Preferably, the surfactants are nonionic or involve mixtures of non-ionic types with a minor proportion,

  up to 30%, of an amphoteric or anionic surfactant.

  Surfactants facilitate processing and are also effective in substantially desizing the fabric, such as starch or other desizing agents. The amount of surfactants typically ranges from about 0.5 to 5.0 g per liter d bath water preferably from 0.5 to 1.5 g per liter of water. In the processes according to the invention, the concentration of the salt can vary so as to increase the efficiency of the dyes used and, consequently, the percentage of exhaustion of the dye on the textile If compared with the single baths according to the invention containing a cellulase enzyme and a direct dye (e.g. Pyrazol Fast Turquoise FBL) at a p H of 4.5 and at a temperature of 60 ° C, increasing the salt concentration by 10 g per liter of liquid of the bath at 20 g per liter of the bath liquid appears to improve the exhaustion of the dye from 84% to 90% It can therefore be seen that the present process can use salt concentrations exceeding those which one would normally think of using or those particularly recommended for a

  use with the particular direct dye chosen.

  At the end of the treatment in the single bath described in the present invention, the denim fabric can optionally be rinsed. The rinses can be rinses with

  hot or cold water and generally more

  rinses One or more of the rinses may also contain a purifier of dye components which may

  to have been released or to have remained in the form of

  siduals in the single bath process These products include those which are commonly known and which are used in this case, such as those which are based on acrylate copolymers or which contain them One of these known products is

  Sandopurel RSK, which is currently available commercially

  especially from Sandoz Chemicals, Basel, Switzerland These pro-

  duits can be used in conjunction with a base such as soda ash and each is typically used in amounts of up to about 3% by weight, based on

dry weight of the articles to be treated.

  After the treatment in the single bath described here, the denim textile can be subjected to other conventional treatment steps. These conventional treatment steps include, for example, finishing steps, such as treatment with softening agents,

finishing, lubricants.

  In one embodiment of the invention there is provided a preparation for the treatment of textile which contains at least one cellulase and a direct dye, and optionally, but preferably, at least one salt, in an amount effective for form an electrolyte Such a preparation for textile treatment is a concentrate which is useful in the

  subsequent formation of a single aqueous treatment bath.

  Said cellulase is preferably a preparation containing cellulase, in particular a preparation containing cellulase of the type which is currently commercially available As indicated above, such preparations containing cellulase commercially available include those which are known to be useful in the textile field for one or more purposes, including as washing aids and as finishing agents. Said direct dye is preferably in the form of one or more direct dyes, such as those which are described in the Color Index As an optional but preferred constituent to be incorporated in the preparation for the treatment of textiles is the salt which is useful in conjunction with the direct dye of the composition Preparations for the treatment of textiles (namely concentrates) can be produced by simple addition of two or more of the constituents, by whatever effective means for producing mixtures For example, when the cellulase enzyme preparation, direct dye, salt and any other optional component are in the form of normally dry solids, measured amounts of the components can be introduced respective in a mixing device, such as a powder mixer, a grinder or a drum, which is then operated for a period sufficient to ensure an intimate mixing of the respective constituents In another example, when one or more of the constituents essential and optional are in the form of a liquid or a semi-solid (paste, gel, etc.), it is preferred to mix independently

  normally dry solid constituents to form a pre-

  dry mix, then mix the liquid or semi-constituents

  solids together to form a liquid premix Then,

  you can combine and mix the dry premix and the pre-

  liquid mixing by any effective means to assure an intimate mixing of the constituents forming the preparation for

  textile processing For example, mixing the pre-

  Dry mixing and liquid premixing can be done through the use of a mixer equipped with an agitator, such as a mechanical paddle stirrer or a magnetic stirring rod. Alternatively, the preparation for textile treatment described above may also contain an amylase enzyme. These may be commercially available amylase preparations and preparations containing amylase and cellulase, including including those known to be useful in the textile field for one or more reasons, including as washing aids and as finishing agents An example of a suitable preparation is

Bactosol MTN.

  The compositions for the treatment of textiles can also comprise optional constituents including, but not limited to, those which have been mentioned above, namely: wetting agents, suspending agents, dispersants, surfactants, leveling agents, buffering agents, as well as other conventional constituents which are not particularly described here One or more of these additives can be added to the compositions for treating textiles according to the invention, in any amount which not found to undesirably limit the

  functioning of cellulase and direct dye.

  The preferred forms of the compositions for treating textiles are those in which the constituents incorporated are normally in dry solid form.

  dry forms of enzyme preparations are known.

  Another preferred form of the composition for

  Textile processing is a form in which the constituents

  kills can normally be in the solid, liquid or semi-solid state, but in which the chosen cellulase enzyme exhibits activity, preferably exhibits its optimal activity, at a p H or in a domain of p H which includes the p H or the p H domain of the direct dye These compositions for the treatment of textiles are expected to have good long-term storage stability.

  what the compositions for treating textiles have

  one or more non-dry solid constituents in the

  what the difference between p H or the domain of p H at which the chosen cellulase enzyme exhibits its activity, preferably

  rence exhibits its optimal activity, and the p H or the p H domain of the direct dye is minimized, also exhibit a

good storage stability.

  It is further understood that when the compositions

  for the treatment of preferred textiles contain

  optional killers, it is preferred that these constituents are present in a normally dry solid form or are present in such amounts, or so that these optional constituents have a p H or a domain of p H such,

  that the overall p H of the composition for the treatment of tex-

  tiles is included within the limits of the active p H of the enzyme

cellulase incorporated therein.

  The single-bath processes according to the invention can be carried out in any apparatus or process which can be used to carry out an enzymatic treatment of

  textiles in jeans or clothing and / or denim goods.

  A useful form of apparatus is the commercial washing machine known for use in one-bath or two-bath processes. Typically, the aqueous textile treatment bath occupies about half the capacity of the machine. machine The articles to be treated, namely denim textiles, clothing and / or denim articles, can be added at the start of the treatment process and are usually present in the machine in an amount making it possible to obtain a weight ratio between items and the treatment bath which ranges from 1: 4 to 1:30, although a range of 1:10 to 1:20 is more common If pumice stones or other materials are to be added abrasives to promote abrasion of the denim fabric, they are usually used at this time Pumice stones or other abrasive materials are typically added to provide a weight ratio between pumice stones or other abrasive materials and th ranging from 0.5: 1 to 1: 4 More

  typically, this range is from 1: 1 to 1: 3.

  At the end of the desizing step of the process (although it does not necessarily follow immediately), water is put in the washing machine, in a measured amount of "hot" water (about 60 ' C) from a water supply

  domestic or commercial hot water and "cold" water (about 1-

  27> C) If the temperature is too low, it can be raised to a sufficient level by an appropriate heating device, such as a heating element which is commonly supplied in the washing machine Once the appropriate temperature is reached then the required quantities of the cellulase enzyme preparation, optionally of the amylase enzyme preparation, of the direct dye and of the salt according to the invention, are added to the water, as well as the other constituents.

  optional, to form the single bath according to the invention.

  During this addition, the processing of the articles begins.

  It is understood that, if amylases and cellulases are used simultaneously in the single-bath process of the invention, no prior desizing step is necessary. Other sequences of addition of the compositions according to the invention are envisaged as forming part of the scope of the invention, such as the addition of less than all of the constituents forming a composition at one time and the subsequent addition of less than all of the remaining constituents or all of the remaining constituents

  a little later Such a sequential addition of the com-

  position may be desirable in certain circumstances,

  such as those that can be envisaged when the enzyme cellu-

  lase and, optionally, the enzyme amylase and others-

  optional constituents (such as buffering agents), but not the

  dye, are added to the bath to allow pre-treatment

  ment of the articles beforehand, in order to confer a washed-out effect, and only then one adds the dye and the other optional constituents remaining in the single bath to start the over-dyeing of the articles a little later In all cases, the dyeing is done at least in the presence of cellulase. Another sequence for implementing the

  single bath process plans to add quantities

  quises of the preparation of cellulase enzyme, of the dye di-

  rect and salt according to the invention, as well as other constituents

  optional kills, then, at a later time, but before the end of the treatment process, the addition of an additional amount of an acid or a base to adjust the p H of the bath, in order to increase the activity of the direct dye and optionally deactivating the cellulase enzyme present In another sequence variant, an additional amount of salt is added before the end of the treatment process to increase the activity of the direct dye In yet another sequence variant, the temperature of the single bath is raised from an initial temperature of the single bath to a higher temperature during the process, namely an increase in temperature to a temperature higher than that at which the enzyme cellulase presents its optimal activity, or a rise in temperature to a temperature where we observe the increase in exhaustion

  dye, in particular a direct dye.

  At the end of the treatment process, the liquid is removed from the articles and the articles are preferably rinsed during one or more rinses. The treatment process with a single bath can be followed by other stages of conventional treatment process. , for example, other washing steps,

rinsing or finishing.

  In one of these rinsing processes, the articles are rinsed in two stages, first by rinsing with water at the temperature of the water used in the previous process and draining, then by rinsing with water at a temperature that is low enough to remove all enzymes

  remaining cellulases entrained in articles.

  An important aspect of the invention is the fact of providing a simultaneous treatment to impart a used appearance and overdyeing in a single bath. Surprisingly, it has been discovered that this object is achieved at temperatures which are not known in the art to be particularly effective for the dyes used In the case of

  the use of a conventional direct dye, which has normal-

  At a dye temperature in the range of 88-94 C, the use of the enzyme cellulase as a dye dye aid has been shown to lower the temperature.

  effective dyeing It has been discovered that these dyes

  rects, which were previously known to be most effective at temperatures of about 88 C and above, are now found to be similarly effective at lower temperatures in the presence of the enzyme cellulase, at temperatures at which the cellulase enzyme is active This effective lowering of the dyeing temperature is typically 17-28 ° C lower than that recommended for the particular direct dye used. Consequently, it is now possible to carry out a single process. bath when you want to wash at the same time

and an overdye.

  The implementation of such a single bath process provides numerous technical advantages, in particular a reduction in the treatment time due to the simultaneous operation of the enzymes present and the direct dye; a reduction in the total energy requirements that are achieved by effectively lowering the temperature at which the direct dye turns out to function, as well as savings in time and material When an amylase is also incorporated, other technical advantages including a reduction in quantities

  starch desizing agents are obtained.

  The articles treated according to the present invention present

  try a uniform dye, which is observed in the over-dyed weft threads, as well as a good exhaustion of the direct dye which is used. In addition, it has been observed that an increase in the salt content increases the exhaustion of the dye. Improving the exhaustion of the dye reduces the amount of dye that must ultimately be discarded and is a technical advantage which is important from the point of view of

  environment and waste treatment.

  The above invention will be more evident if one considers

  refers to the specific embodiments which are shown

  Sentiments of the invention It is nevertheless understood that the particular embodiments described here are provided by way of illustration and are not intended to limit the invention in any way, and it is also understood that the present invention can be implemented. works in a way that is not

  illustrated here, without leaving its frame.

  Exemr) the Exem'ole A 0.77 kg of denim textile in the form of dyed blue jeans are introduced into a Unimac 30 type front-loading washing machine and 0.77 kg of denim textile in the form of textile coupons The denim textile is dyed at the warp threads with conventional indigo and sulfur dyes and the weft threads are not dyed To remove the jeans from the desizing, 28 liters of water are added to the machine. 37.7 C, to which 7.7 g are added

  (or 1% by weight, relative to dry denim textile) from San-

  doclean PCA, which is a conventional nonionic detergent composition (available from Sandoz Chemicals Inc) and 15.4 g (or 2% by weight, relative to the dry jean textile) of

  technical grade soda ash The report arti-

  1:18 keys / liquors The temperature of the water in the machine is raised to 60 ° C thanks to the operation of the integrated heating element of the machine, then the agitator of the machine is started to operate at a "slow" setting for a period of 10 minutes At the slow setting, the agitator operates for 3 seconds, then stops for 12 seconds, each time changing the direction of rotation of the agitator The speed of rotation of the agitator is 30 revolutions per minute Then, for an additional 5 minutes, the machine operates at a "wash" setting, in which the agitator operates for 12 seconds, then stops for 3 seconds, changing every times of direction of rotation of the agitator The speed of rotation of the agitator is 30 revolutions per minute After that, the liquid content of the machine is removed The content of the machine is then subjected to two successive rinsing operations in which 28 liters of water at 37.70 C are introduced into the machine, the machine operates on the washing setting for 3 minutes, after which the liquid content of the machine is removed At this time, any sizing agent present in the articles East

substantially eliminated.

  The single-bath process according to the invention is formed by adding 28 liters of water to the machine at 37.7 ° C., then raising and regulating the temperature of the bath by means of the integrated heating element, at a temperature in the range of 57.2-58.8 C. 7 g (0.25 g / l of bath) of a conventional non-ionic detergent which acts as a wetting agent and 14 g (0 g) are added to the water. , 5 g / l of bath) of 56% acetic acid to adjust the p H to 4.5-5.5 Next, the commercially available cellulase enzymes are added under the name of Bactosol CA, the manufacturer of which indicates that they are optimally active at a temperature of around 55-65 C, in a p H range of 3.8-5.5 In the machine there is a cellulase enzyme at a concentration of 2940 CMC units per pound (0.454 kg) of jeans Subsequently, 560 g (20 g / l of bath) of Glauber salt and 1% by weight (relative to the dry jean textile) of a solution of direct dye of the Lumicrease type are added. Orange 3 LG (Direct Orange 107 from the Color Index) (available from Sandoz Chemicals Inc), which is prepared from a dry form according to the manufacturer's instructions The machine is operated at the "wash" setting for 45 minutes , after which the liquid is removed from the machine We observe that the treated jeans have been effectively over-dyed We also observe that a good exhaustion of the dye is obtained, by visual inspection of a sample of the

  liquid when it leaves the machine.

  At the end of a single bath treatment process, 28 liters of water at 37.7 ° C. are added to the machine and the machine is operated at a "wash" setting for 3 minutes to rinse the textile, after which the liquid is removed from the machine. After rinsing, 28 liters of water at 37.7 ° C. are added to the machine, and then 1% of a conventional polyacrylate containing a soil suspending agent and dye, of the Sandopure RSK type, is added thereto, also available from Sandoz Chemicals Inc The temperature is then raised to 'C by means of the integrated heating element and the machine is started up at the "washing" setting for 5 minutes. The liquid content of the machine is then removed. resulting from this, the jean textile is again rinsed by adding 28 liters of water at 37.7 ° C. and the machine is operated at the "washing" setting for 3 minutes to rinse the textile,

  after which the liquid is removed from the machine.

  Next, the jean textile is treated according to a conventional finishing process. 28 liters of water at 37.7 ° C. and 7.7 g of Ceranine HCA at 1% by weight are added to the machine (relative to the dry jean textile ) (Sandoz Chemicals Inc), which is a conventional cationic finishing agent used to give the textile lubricating, antistatic and softening properties. The machine is run on the "lavagen" setting for 5 minutes at a water temperature of 37.7 C, after

  what we drive the liquid from the machine.

  The denim textile, namely the "blue jean" is removed from the machine and is dried in a conventional domestic dryer, after which the blue jean is removed and inspected It is observed that the denim textile is uniformly dyed, giving a color worn on the previously dyed warp thread, as well as good coloring by the direct dye, evident at the abrasion points, the seams and in the weft thread The articles have both a faded and

  an overdone effect thanks to the single bath process.

  The actual tint intensity is determined by the

  measurement of the exhaustion of the dye, according to the following test.

  Dye exhaustion We get two 20 g pieces of cotton fabric

white bleached.

  In a first laboratory beaker of 500 ml, a piece of textile is placed, to which 495 ml of water at 87.8 C, g (10 g / l of water) of Glauber salt and 1% by weight are added (compared to dry denim textiles) of a solution of direct dye of the Lumicrease Orange 3 LG type (Direct Orange 107 of the Color Index) which was prepared according to the instructions of the

  manufacturer The contents of the beaker are stirred automatically during

  for 45 minutes on a device which continuously rotates the beaker at a speed of 60 revolutions per minute Then,

  remove the textile and we visually observe that all the co-

  lorant du beaker was sold out and deposited on the textile Le

  piece of textile is marked "color indicator" and it has been

  tribute a value of 100%, representative of a complete fixing of the dye by the textile and of an exhaustion of the

dye in the bath.

  In a second 500 ml laboratory beaker,

  produces the other piece of cotton fabric, to which 494 ml of water at 60 ° C are added, 5 g (10 g / l of water) of Glauber's salt, sufficient acetic acid (58%, technical quality ), 0.5 g of Bactosol CA (1 g / l of water) and 1% by weight (relative to the dry jean textile) of a direct dye solution of the Lumicrease Orange 3 LG type (Direct Orange 107 Color Index) which has been prepared according to the manufacturer's instructions. The contents of the beaker are stirred for 45 minutes on a device which continuously rotates the beaker at a speed of 60 revolutions per minute. Then, the textile is removed. The piece is labeled. of textile as a dye exhaustion sample "Using a Chromasensor ACS Model C 55 spectrophotometer, the light reflectance of the textile pieces is measured to obtain a comparison between the relative fixation of the dye in the second laboratory beaker and that of the first laboratory beaker We determine that "the sample dye exhaustion volume "has exhausted 84% of the direct dye in the bath Furthermore, as the bath conditions in the second beaker are as close as possible to the washing machine conditions, it is assumed that the same dye exhaustion occurred in the washing machine and is attributed to exhaustion

  dye in the washing machine worth 84%.

  This test is used to determine the percentage of exhaustion of the dye, because the spectrophotometer cannot accurately read the amount of direct dye absorbed by the denim fabric due to the presence of other dyes used to dye it. origin denim textile.

Example B

  the procedures according to Example A are repeated, except that Lumicrease 3 LG (Direct Yellow 98 from the Color Index) yellow is used as direct dye (available from

  Sandoz Chemicals Inc) in place of the orange Lumicrease 3 LG.

  As in the previous example, we observe that the treated jeans have been effectively dyed with yellow Lumicrease 3 LG We observe that the textile is uniformly dyed, giving a color worn on the warp yarn previously dyed and good coloring by the dye direct evident at the level of

  abrasion points, seams and weft thread.

  The evaluation of the exhaustion of the dye by visual inspection indicates a very good exhaustion of the dye, estimated

greater than 80%.

  Example C, the procedures according to Example A are repeated, except that the violet red Lumicrease 3 LB (Direct Violet 47 of the Color Index) is used as direct dye (available from

  Sandoz Chemicals Inc) in place of the orange Lumicrease 3 LG.

  As in the previous example, we observe that the treated jeans have been effectively over-dyed with red violet Lumicrease 3 LB We observe a good exhaustion of the dye We observe that the textile is uniformly over-dyed, providing a color worn on the warp thread complexion and good coloring by direct dye, evident in

  abrasion points, seams and in the weft thread.

  Dye depletion assessment indicates depletion

80% direct dye.

  Example Dle D the procedures according to Example A are repeated, except that Pyrazol Fast Turquoise FBL (Direct Blue 199 from the Color Index) (available from Sandoz Chemicals Inc) is used as direct dye instead of l 'orange Lumicrease 3 LG As in the previous example, we observe that the treated jeans have been effectively over-dyed with Pyrazol Fast Turquoise FBL We observe a good exhaustion of the dye We observe that the textile is uniformly dyed, providing a color worn on the warp yarn previously dyed and good coloring by direct dye, evident in the

  abrasion points, seams and in the weft thread.

  Dye depletion assessment indicates depletion

84% direct dye.

Example E

  The procedures of the preceding examples are repeated, except that the denim textiles are not desoldered before the single-bath process and that cellulose enzymes commercially available under the name Bactosol are used instead. CA, 1-1.5% by weight (relative to dry denim textile) of a mixture of cellulases and amylases available in

  trade under the name of Bactosol FB fl.

Claims (9)

R E V E N D I C A T I O N S   1 Single-bath process for obtaining a washed-out and overdyed appearance on a dyed denim textile or an article containing a denim textile, comprising the step which consists in bringing the denim textile or the article containing the denim textile into contact jeans with an aqueous bath containing a water-soluble or water-dispersible dye and a cellulase enzyme, under conditions of p H and temperature where the cellulase enzyme exhibits activity for a time sufficient to obtain an appearance of wash and overdye on a dyed denim textile.   2 single-bath method according to claim 1, in   which the cellulase enzyme shows its activity in do-   main of p H of 3.8-6.5 and in the temperature range of 35-   C. 3 A single bath method according to claim 1 or 2, in which the cellulase enzyme exhibits its optimal activity in the p H range of 3.8-5.5 and in the temperature range of 55-65 C .   4 Single bath process according to any of the   previous claims in which the aqueous bath contains also a salt.   A single bath method according to any of the   previous claims in which the dye is a co- lorant direct.   6 Single bath process according to any of the   previous claims in which the aqueous bath contains also an amylase enzyme.   7 Aqueous bath composition for imparting a washed out or overdyed appearance to a denim textile or an article containing a denim textile, which comprises a soluble dye   in water or dispersible in water and a cellulase enzyme.   8 aqueous bath composition according to claim 7,   wherein the dye is a direct dye.   9 aqueous bath composition according to claim 7 or 8, which also includes a salt.   Aqueous bath composition according to any one of   Claims 7 to 9, which also comprises an amylase enzyme.   11 A composition for treating textiles which comprises a cellulase enzyme, a direct dye and a salt, in which the salt is incorporated in an amount exceeding the amount which is normally believed to be useful at 88-94 C, with the amount of dye direct incorporated into the composition for the treatment of textiles.   12 Use of a cellulase enzyme in a single bath process to overdye a dyed denim fabric.